EP2674402A2 - Superhydrophobe Beschichtung - Google Patents

Superhydrophobe Beschichtung Download PDF

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Publication number
EP2674402A2
EP2674402A2 EP13447010.3A EP13447010A EP2674402A2 EP 2674402 A2 EP2674402 A2 EP 2674402A2 EP 13447010 A EP13447010 A EP 13447010A EP 2674402 A2 EP2674402 A2 EP 2674402A2
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Prior art keywords
weight
sio
less
suspension
face
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EP13447010.3A
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English (en)
French (fr)
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EP2674402B1 (de
EP2674402A3 (de
Inventor
Joël De Coninck
Damien Duvivier
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Detandt - Simon Ets
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Detandt - Simon Ets
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3072—Treatment with macro-molecular organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C09C1/30—Silicic acid
    • C09C1/3081—Treatment with organo-silicon compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C09D1/02—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances alkali metal silicates
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1681—Antifouling coatings characterised by surface structure, e.g. for roughness effect giving superhydrophobic coatings or Lotus effect
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/66—Additives characterised by particle size
    • C09D7/69—Particle size larger than 1000 nm
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
    • C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
    • C03C2217/475—Inorganic materials
    • C03C2217/478—Silica
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/76—Hydrophobic and oleophobic coatings

Definitions

  • the present invention relates to a superhydrophobic coating.
  • super hydrophobic coating is understood to mean a coating having an outer surface for which a drop of water (10 ⁇ l) placed on this outer surface in a horizontal position defines a static contact angle of recoil of more than 135 °.
  • more than 140 ° preferably more than 145 °, for example from 145 ° to 160 °
  • a forward contact angle of more than 135 ° preferably more than 140 °, preferably more than 145 °, for example 145 ° to 160 °.
  • the applicant then sought a solution to obtain, in a simple manner, a superhydrophobic surface at a very economical cost, but above all that can be done in a very short time.
  • the thickness of the sub-layer and the outer layer is very low, since it is desired to obtain substantially a single layer.
  • the applicant has therefore sought to obtain a superhydrophobic coating that can already be obtained by the deposition of a single layer of SiO 2 particles, which layer can be thick and which does not require melting of particles on the support.
  • This layer can be deposited in a single step, without the need to deposit a precoat of SiO 2 particles.
  • This coating is therefore easier to deposit and has a greater reliability of its super hydrophobic performance.
  • the pH measurement can be determined using a WTM "Multiline P4" apparatus with a Hamilton LiCl electrode. Such a pH measurement is described in PCT / E2008 / 000065. In the present specification, when reference is made to a pH, this pH is measured at 20 ° C.
  • a coating prepared from such a fresh acidic composition that is to say prepared from a composition in which the solid particles, the alcohol, the TEOS and the acid are put into contact between them less than 12 hours, preferably less than 6 hours, preferably less than 3 hours, composition prepared and maintained at 20 ° C or at a temperature below 20 ° C, it was possible to obtain a superhydrophobic coating, even in the absence of fluorinated compounds, having excellent resistance to acids and other chemicals, but also good abrasion resistance and excellent adhesion to the support.
  • the coating had good mechanical strength, particularly as to its crushing, its detachment. It also had good chemical resistance, even for acidic pH, for example at pH 4 or less, for example acid rain.
  • the coating according to the invention although it consists substantially of a single relatively thick layer, has been found to be excellent for giving better resistance to cracking of the support.
  • the primary SiO 2 nanoparticles of said agglomerates present in the layer outer and having a number average particle size less than 70nm have a particle size dispersion having a fraction of nanoparticles of less than 40nm, or even less than 20nm and a nanoparticle fraction of more than 80nm, or even more than 100nm.
  • the granulometric dispersion of the primary SiO 2 nanoparticles of said agglomerates has a 90% degree of polydispersity greater than 0.2, advantageously greater than 0.5, preferably greater than 0.7, more specifically greater than 1 .
  • the coating according to the invention is prepared from a fresh acid suspension whose water / Teos molar ratio is between 0.8 and 1.2, while the amount of Teos is such that the weight ratio Teos / solid particles is between 2 and 5.
  • the subject of the invention is also a product in which a face or a primary layer covering this face has a resistance to the acid medium of the suspension described above, for at least 1 minute, said face or primary layer being provided with a coating according to the invention, as described above, in particular as described in any of the appended claims.
  • the product can be any product. If the face of the product to be coated with the super hydrophobic coating according to the invention does not contain a silicon atom or not enough Si atoms, it is preferable to provide said face with a primary layer comprising Si, in particularly in the form of SiO 2 , a primary layer having a resistance to the acid medium of the fresh acid suspension to form the coating according to the invention.
  • said face before applying the suspension on one side of the product, is provided with a primary layer having a resistance to the acid medium of the suspension, this primary layer comprising silicon atoms, in particular SiO 2 particles.
  • the suspension is kept below 20 ° C, it may be applied for more than 12 hours after preparation. If the suspension is maintained at a temperature above 30 ° C, it is preferable to use the suspension less than 3 hours, especially less than one hour after mixing Teos with the acid in the presence of water.
  • said composition and said aqueous acidic medium are simultaneously projected to said face, so as to ensure the mixing of said composition with said acid medium to form a suspension as defined in claim 1 at least on said face.
  • the method according to the invention advantageously comprises one or more of the characteristics of the coating according to the invention as given above and / or as claimed.
  • the application of the suspension on the face or on the primary layer may be carried out by brush, brush or roller, by immersing the support in a bath, leaving the suspension cast along the face or primary layer, by spraying, for example by means of an Air Brush spraying apparatus, model 360 of Badger.
  • compositions may be used, for example a first non-acidic composition comprising TEOS and a second acidic aqueous composition not containing TEOS, which are either mixed together just before being sprayed. or separately sprayed to form a mixture during the spraying step (e.g., prior to contacting the compositions with the face to be coated, or upon or after contact of the compositions with the face to be coated .
  • Silica 1 hydrophobic synthetic amorphous silica of average particle size in a number equal to about 40 nm (particle size of the primary particles measured by transmission electron microscope, TEM, Phillips, CM360). The particles are white in color and surface-treated to exhibit dimethyl siloxy functions.
  • the BET specific surface area of the particles is between 110 and 140 m 2 / g (method described in paragraph 0051 of US2010 / 0196811 - DIN EN ISO 9277 / DIN 66132).
  • the relative residual content of the SiOH group (with respect to the silanol content of the hydrophilic pyrogenic silica, which is about 2 SiOH groups per nm 2 ) is about 50%, i.e.
  • the relative silanol content for the hydrophobic silica is about 1 SiOH group per nm 2 .
  • the relative residual content of SiOH group surface is, for example, determined by the method referred to in paragraph 0047 of US2010 / 0196811 published on August 5, 2010 or paragraph 0161 of US2007 / 0281878 i.e. by acid-base titration by GW Sears, Anal. Chem., 1956, 28, 1981 and 12, 1950.
  • the carbon content of the particles is less than 2% (content measured by the method described in paragraph 0162 of US2007 / 281878 that is, by elemental carbon analysis, by burning a sample at more than 1000 ° C in a stream of oxygen, and by detecting and quantifying the CO 2 produced using infra-red detectors, for example from the apparatus LECO 244 marketed by Leco Corporation, MI, USA.
  • a 4% dispersion by weight of particles dispersed in a liquid medium consisting of 50% by weight of water and 50% by weight of methanol has a pH of about 4.5.
  • Such particles are marketed under the name HDK H13L - Pyrogenic Silica by Wacker-Chemie, Germany.
  • the particles used had a measured degree of polydispersity of 0.5.
  • Silica 2 hydrophobic synthetic amorphous silica of average particle size equal to about 40 nm (particle size of the primary particles measured by transmission electron microscope, TEM, Phillips, CM360). The particles are white in color and surface-treated to exhibit dimethyl siloxy functions. The BET specific surface area of the particles is between 170 and 230 m 2 / g. The relative residual content of SiOH group surface (based on the silanol content of the hydrophilic pyrogenic silica, which is about 2 SiOH groups per nm 2 ) is about 25%, i.e. the relative silanol content for the hydrophobic silica is about 0.5 SiOH group per nm 2 .
  • the carbon content of the particles is less than 2%.
  • a dispersion at 4% by weight of particles dispersed in a liquid medium consisting of 50% by weight of water and 50% by weight of methanol has a pH of about 4.5.
  • Such particles are marketed under the name HDK H20 - Pyrogenic Silica by Wacker-Chemie, Germany. The particles used had a measured degree of polydispersity of 0.7.
  • Silica 3 with negative charge hydrophilic synthetic amorphous silica of average particle size equal to about 40 nm (particle size of the primary particles measured by transmission electron microscope - Transmission Electron TEM microscope, Philipps, CM200).
  • the particles are white in color and have a BET surface area of about 125 m 2 / g.
  • the particles are treated with polydimethylsiloxane.
  • the relative residual content of the SiOH group (with respect to the silanol content of the hydrophilic pyrogenic silica, which is about 2 SiOH groups per nm 2 ) is less than 25%, i.e. the relative silanol content for the hydrophobic silica is less than 0.5 SiOH group per nm 2 .
  • the carbon content of the particles is less than 3%.
  • a dispersion at 4% by weight of particles dispersed in a liquid medium consisting of 50% by weight of water and 50% by weight of methanol has a pH of about 4 to 5.
  • Such particles are marketed under the name HDK H13TD - Pyrogenic Silica by Wacker-Chemie, Germany.
  • the particles used had a measured degree of polydispersity of 0.5.
  • compositions were prepared which were then applied in a single operation to a previously cleaned glass surface. Two minutes after applying the composition to the glass surface, the treated surface was rinsed with ethanol and the treated surface was dried at 60 ° C for 10 minutes.
  • the static back contact angle and the forward static contact angle were then measured for each of the treated and dried surfaces to determine whether it is much greater than 135 °.
  • the slip angle was also measured by determining the inclination to be given to the surface of the coating with respect to a horizontal plane, so that a drop of water of 10 ⁇ l flows downwards.
  • a silica dispersion was prepared by mixing the silica in the alcohol. This dispersion was then added to TEOS. Finally, the acid, optionally premixed, was added to a quantity of ethanol and / or methanol. This dispersion was subjected to an ultrasound homogenization phase for 5 minutes after the addition of the acidic medium.
  • the following table shows the composition of the dispersions prepared, the time T elapsed between the addition of the acid medium to the mixture and the application of the dispersion or suspension on the glass surface, as well as the static contact angles of recoil and advancement ( ⁇ recoil, ⁇ advancement), and the slip angle.
  • the slip angle was very low. For these coatings, less than 5 ° was indicated, even if the measured angle was closer to 1 to 2 °. For coatings not according to the invention, the slip angle is greater than 20 °.
  • the TEOS will form a layer around the SiO 2 particles, this layer adhering to the particles via the still existing silanol sites. SiO 2 bonds will thus be formed between silica atoms of adjacent particles, but also between the particles and silica atoms of the glass support.
  • the coating corresponding to the dispersion or suspension 1 it was determined whether the coating exhibited porosity for ambient humidity. This determination was carried out by means of an atmospheric porosimeter ellipsometer (EPA marketed by Semilab Sopra, Courbevoie, France) which gives a moisture adsorption-desorption curve at 20 ° C., curve defined by the angle Phi of the tangent. To do this, the coating is placed in an atmosphere whose humidity varies. The adsorption-desorption curves overlap, thus indicating that the superhydrophode coating according to the invention does not absorb moisture.
  • an atmospheric porosimeter ellipsometer EPA marketed by Semilab Sopra, Courbevoie, France
  • the roughness of the coating corresponding to the dispersion or suspension 1 was characterized by a Wenzel factor of 1.28 measured with a magnification of 50, by an AFM apparatus using SPIP software.
  • the thickness of this coating corresponding to the suspension or dispersion 1 was approximately 1 ⁇ m.
  • Dispersion 1 was prepared again, but the mixture was operated at 15 ° C by ultrasound. The dispersion was very homogeneous. The coating obtained by means of this dispersion 1 more homogeneous (by application 20 minutes after the beginning of the mixing phase) was a coating similar to the coating according to the invention of the table above, but having a greater homogeneity.
  • the coatings according to the invention had good resistance to abrasion, but also to various chemical agents.
  • the figure 1 schematically shows steps for providing a face of a support with a coating according to the invention.
  • Step 0 cleaning and degreasing of the surface to be provided with a superhydrophobic coating.
  • Step 1 The face to be provided with a superhydrophobic coating is tested to evaluate its resistance to the acid medium of the suspension.
  • Step 2 control of resistance to acid medium and / or other properties of the face
  • the face of the support is provided with a primary layer resistant to the acid medium for at least 5 minutes.
  • Such a primary layer can be deposited on said face by using numerous compositions, in particular compositions containing silicone. or siloxane, with methods such as spraying, brushing, dipping the material into a bath, vapor deposition, and the like.
  • SILIKOPON EF epoxy silicone hybrid binder sold by Evonik Tego Chemie GmbH, Germany can be used. This hybrid binder is advantageously applied after addition of dispersing agent and crosslinking or curing agent (Dynasilan Ameo (R)). Details of such formulations are given on the site of the company EVONIK TEGO CHEMIE.
  • This primary layer is for example applied at ambient temperature.
  • Step 4 Application of a suspension on the acid-resistant side or on the primary layer
  • Brush or suspension brush 1 or 4 of the previous table is applied to the face or the primary layer.
  • the coated side of the suspension is washed with an alkaline solution, advantageously acidic, to remove the particles which do not sufficiently adhere to the support.
  • This washing step can also be carried out by steam jet.
  • this drying can be carried out at room temperature, the drying is advantageously carried out at a temperature of 30 to 60 ° C, for example in a radiation-inert chamber.
  • the drying can consist only of a treatment by means of a chamois leather.
  • Step 8 Quality control
  • the method according to this example is shown schematically in figure 2 .
  • a first alcoholic composition comprising silica particles and TEOS is prepared on the one hand, this first composition I being substantially free of water, and on the other hand a second alcoholic composition II comprising: acid and water.
  • compositions I and II once mixed, then form a suspension according to the invention, for example suspension 1 or 4.
  • compositions I and II intended to be mixed together to form a suspension 1 or 4 are given in the following table.
  • suspension composition I Composition II 1 2g silica 1 1 ml HCl 37% 50ml alcohol 1 (aqueous solution) 6ml TEOS 1 2g Silica 1 1ml HCl 37% 40ml alcohol 1 10ml alcohol 1 6ml TEOS 1 2g Silica 1 1ml HCl 37% 30ml Alcohol 1 20ml alcohol 1 6ml TEOS 4 1g Silica 1 1ml HCl 37% 50ml alcohol 1 6ml TEOS 4 1g Silica 1 1ml HCl 37% 30ml alcohol 1 20ml alcohol 6ml TEOS 4 1g Silica 1 1ml HCl 37% 20ml alcohol 6ml TEOS 4 1g Silica 1 1ml HCl 37% 20ml alcohol 1 30ml alcohol 1 6ml TEOS 4 1g Silica 1 1ml HCl 37% 20ml alcohol 1 30
  • step 4 is replaced by the following steps:
  • Step 4A application of the acidic medium (composition II) on the face or primary layer, for example by spraying or brushing
  • Step 4B Application of Composition I on the Face or Primary Coat Wet by Composition II
  • step 4A only a part of the composition II is used, the other part of the composition II being sprayed onto the face after application of the composition I.
  • step 4A the application of the acid medium (step 4A) (optionally with a composition portion II) is performed on the face or primary layer on which the composition It is applied (Step 4B).
  • Example 3 the method of Example 3 is repeated, except that the compositions I and II are sprayed simultaneously on said face or primary layer so that the compositions I and II are in contact with one another. with each other before touching said face or primary layer.
  • the face or primary layer is first treated with a part of the composition II (Step 4bis) before the composition I and the rest of the composition II are projected simultaneously on the face or primary layer.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Nanotechnology (AREA)
  • Wood Science & Technology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Dispersion Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Paints Or Removers (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Silicon Compounds (AREA)
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EP13447010.3A 2012-06-13 2013-06-12 Superhydrophobe Beschichtung Active EP2674402B1 (de)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
BE201200390A BE1020749A3 (fr) 2012-06-13 2012-06-13 Revetement superhydrophobe.

Publications (3)

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EP2674402A2 true EP2674402A2 (de) 2013-12-18
EP2674402A3 EP2674402A3 (de) 2014-02-26
EP2674402B1 EP2674402B1 (de) 2020-05-13

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104212346A (zh) * 2014-09-05 2014-12-17 东莞市瀛通电线有限公司 疏油疏水耐沾污涂层材料的制备方法、制品及应用

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040175579A1 (en) 2003-03-05 2004-09-09 Smith David A. Method for chemical vapor deposition of silicon on to substrates for use in corrosive and vacuum environments
US20070281878A1 (en) 2004-03-25 2007-12-06 Wacker Chemie Ag Particle-Stabilised Emulsions
US20100196811A1 (en) 2007-07-18 2010-08-05 Wacker Chemie Ag Highly disperse metal oxides having a high positive surface charge

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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